Refereed journal article or data article (A1)

One-Pot Synthesis of Menthol from Citral over Ni/H-β-38 Extrudates Containing Bentonite Clay Binder in Batch and Continuous Reactors

List of AuthorsSimakova Irina L.,Vajglová Zuzana,Martínez-Klimov Mark, Eränen Kari, Peurla Markus, Mäki-Arvela Päivi, Murzin Dmitry Yu

PublisherAmerican Chemical Society

Publication year2023

JournalOrganic Process Research and Development

Journal name in sourceOrganic Process Research and Development

Volume number27

Issue number2

Start page295

End page310




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Optimization of bifunctional Ni catalysts was performed to enhance the catalytic performance in the one-pot synthesis of commercially valuable menthol from citral. The effect of nickel precursors (nitrate, chloride, acetate, and sulfate) and the addition of bentonite clay was investigated in citral transformations in a batch reactor at 70 °C and 10 bar hydrogen, demonstrating higher activity for the Ni-H-β-38-bentonite composite derived from a nickel nitrate precursor, which can be attributed to a higher surface area, optimal Brønsted to Lewis acidity and metal particle size, as well as the egg-shell distribution of Ni particles. H-β-38 impregnated with nickel nitrate, followed by calcination and reduction, was shaped with bentonite as a binder to give extrudates for exploring the citral transformations in the trickle-bed reactor at 50–70 °C and 10 bar hydrogen. The highest selectivity to the desired menthols of 45% was obtained with 70% stereoselectivity to the menthol isomer at 70 °C. The apparent activation energy for citral transformations to menthols of 18.6 kJ/mol indicated the presence of mass transfer limitations. Catalytic activity was linked with the physical-chemical properties, which were characterized by transmission electron microscopy, X-ray diffraction, temperature-programmed reduction, Fourier transform infrared spectroscopy with pyridine, N2 physisorption, and inductively coupled plasma–optical emission spectrometry methods.

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Last updated on 2023-28-03 at 16:55